CN101269973B - Method for synthesizing nano-scale oxide ceramic powder body - Google Patents
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Abstract
The present invention belongs to the technology of preparing ultra-fine nano powder and in particular discloses a synthetic method of preparing nano oxide ceramic powder. In the method, sugar is added for pyrolysis. Under the atmospheric conditions, a metal ion source is dissolved in an appropriate solvent; sugar and foamer ammonium nitrate are added; the prepared solution is dried; and the prepared substance is pre-sintered at a lower temperature to synthesize the nano powder. The synthetic method requires no high-temperature sintering, inhibits the generation of agglomeration and excessive growth of grains, and can prepare the ceramic powder with the grain size of 10 to 90nm, uniform distribution of grains, high sintering activity, and uniform and stable ingredients. The synthetic method has universality for preparing various oxide nano powder, and can be used for preparing powder only by using the appropriate solvent to dissolve the metal ion source; and the prepared powder has higher chemical activity in wider application range.
Description
Technical field
The invention belongs to the ultra-fine nano-powder technology of preparing, particularly relate to a kind of synthetic method of nano-scale oxide ceramic powder body.
Background technology
Oxide ceramic powder body is as the raw material of the multiple pottery of preparation, and its purity and fineness have direct influence for the performance and the quality of ceramic components especially electronic component.Along with the high speed development of electronic devices and components to high integration, high precision, high reliability, multi-functional and miniaturization, industrial purity for powder, particle size, moulding and sintering characteristic are had higher requirement.Therefore developing high-purity, ultra-fine, granule-morphology ideal ceramic powder has broad application prospects and the important strategic meaning.
The preparation method of ceramic powder mainly comprises solid phase method, the precipitator method, sol-gel method, hydrothermal method, evaporation-coacervation and gas-phase reaction method.
Solid phase method is because based on the solid state reaction principle, the chemical ingredients homogeneity of powder is difficult to guarantee, simultaneously owing to need high-temperature calcination and ball milling repeatedly, prepared powder has characteristics such as particle size distribution broad, particle shape is inhomogeneous, purity is low, is difficult to obtain the high quality powder high-purity, ultra-fine, that distribution of sizes is very narrow.Evaporation-coacervation and gas-phase reaction method can obtain that particle diameter is little, component homogeneous high purity powder, but equipment complexity, cost height still do not have industrial application value.The preparation method of high quality ceramic powder focuses mostly on the methods such as the precipitator method, sol-gel method and hydrothermal method that with the liquid phase reaction are principal character at present.
It is raw material that sol-gel method adopts metal alkoxide, and hydrolysis in organic medium, condensation make alkoxide solution obtain gel through the sol-gel process, obtain superfine powder through super-dry and calcination processing again.Powder has the purity height, forms the characteristics even, that granularity is little, chemically reactive is strong, but because will be through 600～1000 ℃ of calcinings, powder is very easily reunited, and the operational condition requirement is very strict, and raw-material costing an arm and a leg is difficult to scale operation in industry.
Hydrothermal method is constructed and crystal growth by the particulate of the realization of the chemical reaction under the suitable hydrothermal condition in sealed pressure vessel atom, molecular level, it is strong that prepared powder has polarizability, powder crystal grain is grown complete, particle diameter is little and be evenly distributed, the reunion degree is little, active advantages of higher in sintering process is the prefered method of a large amount of high-level powders of current preparation.But (30～50MPa), energy consumption is big, and the direction of current hydrothermal method development is to reduce temperature of reaction and reaction pressure for temperature of reaction that the preparation process of hydrothermal method is had relatively high expectations (200～500 ℃) and very high pressure.
Method effective at present, ripe, that be easy to produce in enormous quantities mainly is chemical coprecipitation and high-temperature spray pyrolysis method.Chemical coprecipitation utilizes chemical reaction exactly in solution, obtain the precipitation of metal hydroxides or difficulty soluble salt.These throw outs must change required ceramic oxide powder into through pyroprocessing.During this time, often exist, and next step water washing cleaning and dehydration are all caused very big difficulty with a kind of gel form for a lot of oxyhydroxide that obtain.The powder of dehydration and high-temperature process produces reunites, and causes the performance rapid deterioration.Spray pyrolysis is to adopt the solution of metal-salt at high temperature forming the droplet thermal degradation by spraying equipment, forms fine powder.The benefit of this method is that technology is simple, is easy to control, but apparatus expensive, the decomposition temperature height, particle diameter of nanometer powder is bigger.If can get up the advantages of two kinds of methods, under lower temperature, realize the preparation of oxide ceramic powder body, so, the raising and actual generation of the performance of powder are used and will be had great importance.
Summary of the invention
The purpose of this invention is to provide that a kind of technology is simple, cost is low, be convenient to operate and the method for the manageable a kind of synthesizing nano-scale oxide ceramic powder body of preparation process, to overcome the deficiency of chemical coprecipitation and spray pyrolysis, in conjunction with both advantages, under lower temperature, realize the preparation of oxide ceramic powder body, the raising and actual generation of the performance of powder are used and will be had great importance.
The method of described synthesizing nano-scale oxide ceramic powder body, it is characterized in that, this method adopts the sugaring pyrolysis method to prepare nano-scale oxide ceramic powder body, under condition of normal pressure, metal ion source is dissolved in the solvent, adds sugar and whipping agent ammonium nitrate, again with resulting solution drying, the material that obtains is pre-burning synthesis of nano powder at a lower temperature
Relative proportion between the described metal ion source is according to the elementary composition decision of prepared product, and its processing step is:
1) under 20～90 ℃ of temperature condition, metal ion source is dissolved in the solvent fully, obtains A liquid;
2) in A liquid, add sugar, under 20～160 ℃ of temperature, stir, make dissolving fully, obtain B liquid;
3) add ammonium nitrate in B liquid, heated and stirred makes dissolving;
4) the black bulk material C of carbonization will be obtained behind the gained liquid convection drying;
5) with C pre-burning 2～6h under 200～900 ℃ temperature, synthesis of nano powder.
Described metal ion source is one or more mixtures in nitrate, vitriol, muriate, organo-metallic alkoxide, metal ion complex and the colloidal sol that contains metal ion.
Described solvent is the one or more kinds of mixtures in water, ethanol, methyl alcohol, propyl alcohol, Virahol, butanols, isopropylcarbinol, acetone, ethylene glycol, glycerine and the methyl ethyl diketone.
Described sugared add-on is (0.1～20) with respect to the molar ratio of ionizable metal salt in the system: 1.
The add-on of described ammonium nitrate is (0.1～20) with respect to the molar ratio of the ionizable metal salt in the system: 1.
Described convection drying is in thermostatic drying chamber, 100～290 ℃ of drying temperatures, time of drying 2～24h.
The invention has the beneficial effects as follows: in metal ion source solution, add sugar; utilize sugar dehydration carbonization at high temperature to form network structure; this network structure forms sterically hindered; new pyrogenous origin nanoparticle is formed effective catch net; they are kept apart, thereby avoided the reunion of powder and growing up of crystal grain.The vesicular carbon of sugar charcoal formation has very high chemically reactive, and the decomposition temperature of metal-salt is reduced significantly.Ammonium nitrate can make the temperature of deviating from of carbon reduce significantly.Thereby can be under lower temperature the synthesis oxide nano-powder.
Utilize synthetic method of the present invention to obtain the high pure and ultra-fine ceramic powder under lower calcined temperature, the grain-size of this powder is between 10～90nm, and grain morphology is even, and distribution of sizes narrow range, sintering activity height, composition are uniform and stable controlled.In addition, with respect to the synthetic method under other normal pressures, synthetic method of the present invention need not washing, need not to introduce foreign ion, thus the purity height of synthetic powder.Need not high-temperature calcination, avoided grain growth and reunion, kept high reactivity.With respect to hydrothermal synthesis method, need not the supercritical state of High Temperature High Pressure, simplified technology, greatly reduce equipment requirements, make the more easy to operate and control of whole process of preparation.And present method has very big universality, and every raw material can dissolve the material that forms solution can obtain corresponding product by this method.
Description of drawings
Fig. 1 is the XRD material phase analysis figure of embodiment 1 powder.
Fig. 2 is the stereoscan photograph of embodiment 1 powder.
Fig. 3 is the XRD material phase analysis figure of embodiment 2 powders.
Fig. 4 is the stereoscan photograph of embodiment 2 powders.
Fig. 5 is the XRD material phase analysis figure of embodiment 3 powders.
Fig. 6 is the stereoscan photograph of embodiment 3 powders.
Fig. 7 is the XRD material phase analysis figure of embodiment 4 powders.
Fig. 8 is the stereoscan photograph of embodiment 4 powders.
Embodiment
The invention provides that a kind of technology is simple, cost is low, be convenient to operate and the method for the manageable a kind of synthesizing nano-scale oxide ceramic powder body of preparation process.Below in conjunction with embodiment this invention is described further:
Choose tetrabutyl titanate (Ti (OC
4H
9)
4), Bismuth trinitrate (Bi (NO
3)
35H
2O), SODIUMNITRATE (NaNO
3) be titanium source, bismuth source and sodium source, glycerol is as solvent.
With 13.614g tetrabutyl titanate (Ti (OC
4H
9)
4) be dissolved in 20mL dehydrated alcohol dilution after, be added drop-wise in the 40mL glycerol, stir under the room temperature and make the thorough mixing dissolving.Take by weighing 9.7014g Bismuth trinitrate (Bi (NO
3)
35H
2O), 1.6998g SODIUMNITRATE (NaNO
3), add successively in the above-mentioned solution, be heated to 40 ℃, vigorous stirring makes dissolving fully simultaneously, obtains metal salt solution A.Take by weighing 21.6g sugar, be dissolved in the A liquid, reconcile solution temperature to 60 ℃, vigorous stirring simultaneously is so that fully dissolving of sugar.After obtaining yellow sticky shape liquid, take by weighing 1.6008g ammonium nitrate (NH
4NO
3), stirring and dissolving.Resulting solution behind dry 24h under 190 ℃, at 500 ℃ of following pre-burning 6h, is obtained bismuth-sodium titanate (Bi
0.5Na
0.5TiO
3) nano-powder.Show that from XRD result the gained powder is the micro mist of perovskite structure, from the SEM photo, finished product belongs to the crystalline particle of the even subglobular of shape, as shown in Figure 1, 2, the particle diameter that shows institute's synthetic powder from XRD particle size analysis and SEM morphology observation is the powder of nanoscale below 100nm.
Select for use tetrabutyl titanate as the titanium source, dehydrated alcohol is as solvent.
Under the room temperature 17g tetrabutyl titanate is dissolved in the dilution of 40mL dehydrated alcohol and obtains solution A, add 27g sugar in A liquid, reconcile temperature to 60 ℃, vigorous stirring makes dissolving fully.After obtaining yellow sticky shape liquid, take by weighing 2g ammonium nitrate (NH
4NO
3), stirring and dissolving.The resulting solution dry 4h under 69 ℃ of elder generation is removed most of solvent, transfer to dry 24h in 190 ℃ of loft drier again.Descending 2～6h to carry out powder at 300 ℃, 500 ℃, 600 ℃, 700 ℃ and 900 ℃ respectively synthesizes.
Shown in Fig. 3,4, XRD forms purified anatase octahedrite phase when showing 300 ℃, and 700 ℃ form purified rutile phase, and middle two temperature spots are two-phase coexistent.XRD particle size analysis and SEM show that diameter of particle is about 50nm.
Embodiment 3 preparation titanic oxide nanos (water)
With the stable titanium tetrachloride (TiCl of alcohols
4) as the titanium source, use deionized water as solvent.
The 380g titanium tetrachloride is dissolved in the 400mL dehydrated alcohol, obtains the stable titanium tetrachloride solution of 548g.Take by weighing aforementioned stable solution 2.73582g, be dissolved under the room temperature in the 10mL deionized water and obtain solution A.Take by weighing 10.8g sugar, stir in the adding A liquid and make dissolving.Take by weighing 1g ammonium nitrate (NH
4NO
3), stirring and dissolving.The resulting solution dry 4h under 105 ℃ of elder generation is removed most of solvent, transfer to dry 24h in 190 ℃ of loft drier again.It is synthetic to carry out powder at 300 ℃, 500 ℃, 700 ℃ and 900 ℃ of following pre-burning 6h respectively.
Shown in Fig. 5,6, the XRD structural analysis show 300 ℃ with 500 ℃ of anatase octahedrites that all can obtain the well-crystallized mutually, 900 ℃ form purified rutile phases, 700 ℃ then is two-phase coexistent.XRD particle size analysis and SEM show that diameter of particle is about 40nm.
Embodiment 4 preparation yttrium aluminum garnet (Y
3Al
5O
12, YAG) nano-powder
Choose Yttrium trinitrate (Y (NO
3)
35H
2O) and aluminum nitrate (Al (NO
3)
3) as raw material, deionized water is as solvent.
Take by weighing 5.74515g Yttrium trinitrate and 9.37825g aluminum nitrate, be dissolved in and obtain A liquid in the 40mL deionized water.Take by weighing 21.6g sugar, stir in the adding A liquid and make dissolving.Take by weighing 1.6008g ammonium nitrate (NH
4NO
3), stirring and dissolving.The resulting solution dry 4h under 105 ℃ of elder generation is removed most of solvent, transfer to dry 24h in 190 ℃ of loft drier again.Carrying out powder at 500 ℃, 600 ℃, 700 ℃, 900 ℃, 1250 ℃ following pre-burning 6h respectively synthesizes.
Shown in Fig. 7,8, the XRD structural analysis shows, has formed the YAG phase in the time of 500 ℃, 600 ℃, 700 ℃, forms the sufficient purified YAG phase of crystallization in the time of 900 ℃.This synthesis temperature is compared with additive method has tangible reduction at 1250 ℃ of synthetic identical powders.XRD and SEM show that diameter of particle is below 100nm.
Claims (4)
1. the method for a synthesizing nano-scale oxide ceramic powder body is characterized in that, specifically prepares bismuth-sodium titanate Bi
0.5Na
0.5TiO
3Nano-powder technology is as follows,
Choose tetrabutyl titanate Ti (OC
4H
9)
4Be titanium source, Bismuth trinitrate Bi (NO
3)
35H
2O is bismuth source and SODIUMNITRATE NaNO
3Be the sodium source, glycerol is as solvent;
With 13.614g tetrabutyl titanate Ti (OC
4H
9)
4After being dissolved in the dilution of 20mL dehydrated alcohol, be added drop-wise in the 40mL glycerol, stir under the room temperature and make the thorough mixing dissolving; Take by weighing 9.7014g Bismuth trinitrate Bi (NO
3)
35H
20,1.6998g SODIUMNITRATE NaNO
3, add successively in the above-mentioned solution, be heated to 40 ℃, vigorous stirring makes dissolving fully simultaneously, obtains metal salt solution A;
Take by weighing 21.6g sugar, be dissolved in the A liquid, reconcile solution temperature to 60 ℃, vigorous stirring simultaneously so that fully dissolving of sugar, obtain yellow sticky shape liquid after, take by weighing 1.6008g ammonium nitrate NH
4NO
3, stirring and dissolving behind dry 24h under 190 ℃, at 500 ℃ of following pre-burning 6h, obtains bismuth-sodium titanate Bi with resulting solution
0.5Na
0.5TiO
3Nano-powder; Show that from XRD result the gained powder is the micro mist of perovskite structure, from the SEM photo, finished product belongs to the crystalline particle of the even subglobular of shape, and the particle diameter of institute's synthetic powder is below 100nm.
2. the method for a synthesizing nano-scale oxide ceramic powder body is characterized in that, it is as follows specifically to prepare titanic oxide nano technology,
Select for use tetrabutyl titanate as the titanium source, dehydrated alcohol is as solvent;
Under the room temperature 17g tetrabutyl titanate is dissolved in the dilution of 40mL dehydrated alcohol and obtains solution A, add 27g sugar in A liquid, adjust the temperature to 60 ℃, vigorous stirring makes dissolving fully, obtain yellow sticky shape liquid after, take by weighing 2g ammonium nitrate NH
4NO
3, stirring and dissolving, with resulting solution earlier 69 ℃ down dry 4h remove most of solvent, transfer to dry 24h in 190 ℃ of loft drier again, respectively 300 ℃, 500 ℃, 600 ℃, 700 ℃ and 900 ℃ down 2～6h to carry out powder synthetic;
XRD forms purified anatase octahedrite phase when showing 300 ℃, 700 ℃ form purified rutile phase, and middle two temperature spots are two-phase coexistent; XRD particle size analysis and SEM show that diameter of particle is 50nm.
3. the method for a synthesizing nano-scale oxide ceramic powder body is characterized in that, it is as follows specifically to prepare titanic oxide nano technology,
With the stable titanium tetrachloride TiCl of alcohols
4As the titanium source, use deionized water as solvent;
The 380g titanium tetrachloride is dissolved in the 400mL dehydrated alcohol, obtains the stable titanium tetrachloride solution of 548g, take by weighing aforementioned stable solution 2.73582g, be dissolved under the room temperature in the 10mL deionized water and obtain solution A;
Take by weighing 10.8g sugar, stir in the adding A liquid and make dissolving; Take by weighing 1g ammonium nitrate NH
4NO
3, stirring and dissolving, with resulting solution earlier 105 ℃ down dry 4h remove most of solvent, transfer to dry 24h in 190 ℃ of loft drier again, it is synthetic to carry out powder at 300 ℃, 500 ℃, 700 ℃ and 900 ℃ of following pre-burning 6h respectively;
The XRD structural analysis show 300 ℃ with 500 ℃ of anatase octahedrites that all obtained the well-crystallized mutually, 900 ℃ form purified rutile phases, 700 ℃ then is two-phase coexistent, XRD particle size analysis and SEM show that diameter of particle is 40nm.
4. the method for a synthesizing nano-scale oxide ceramic powder body is characterized in that, specifically prepares yttrium aluminum garnet Y
3Al
5O
12, YAG nano-powder technology is as follows,
Choose Yttrium trinitrate Y (NO
3)
35H
2O and aluminum nitrate Al (NO
3)
3As raw material, deionized water is as solvent;
Take by weighing 5.74515g Yttrium trinitrate and 9.37825g aluminum nitrate, be dissolved in and obtain A liquid in the 40mL deionized water;
Take by weighing 21.6g sugar, stir in the adding A liquid and make dissolving, take by weighing 1.6008g ammonium nitrate NH
4NO
3, stirring and dissolving is removed most of solvent with the resulting solution dry 4h under 105 ℃ of elder generation, transfers to dry 24h in 190 ℃ of loft drier again; Carrying out powder at 500 ℃, 600 ℃, 700 ℃, 900 ℃, 1250 ℃ following pre-burning 6h respectively synthesizes;
The XRD structural analysis shows, formed the YAG phase in the time of 500 ℃, 600 ℃, 700 ℃, form the sufficient purified YAG phase of crystallization in the time of 900 ℃, this synthesis temperature is compared with additive method has tangible reduction at 1250 ℃ of synthetic identical powders, and XRD and SEM show that diameter of particle is below 100nm.
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| CN103833377A (en) * | 2014-03-21 | 2014-06-04 | 景德镇陶瓷学院 | Particle size control method of ceramic powder prepared by wet chemical method |
| CN114702011B (en) * | 2022-03-17 | 2023-08-25 | 华中科技大学 | Preparation method of two-dimensional non-layered metal oxide porous nano-sheet |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410388A (en) * | 2002-12-06 | 2003-04-16 | 清华大学 | Method of synthesizing nano grade calcium titanium ceramic powder |
| WO2006015692A1 (en) * | 2004-08-12 | 2006-02-16 | Degussa Ag | Yttrium-zirconium mixed oxide powder |
| CN101112973A (en) * | 2007-07-10 | 2008-01-30 | 兰州大学 | Sol-gal process for preparing metal-oxide powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410388A (en) * | 2002-12-06 | 2003-04-16 | 清华大学 | Method of synthesizing nano grade calcium titanium ceramic powder |
| WO2006015692A1 (en) * | 2004-08-12 | 2006-02-16 | Degussa Ag | Yttrium-zirconium mixed oxide powder |
| CN101112973A (en) * | 2007-07-10 | 2008-01-30 | 兰州大学 | Sol-gal process for preparing metal-oxide powder |
Non-Patent Citations (2)
| Title |
|---|
| 齐建全等.钛酸钡纳米粉体的溶液直接合成法.钛工业进展20 3.2003,20(3),25-27页. |
| 齐建全等.钛酸钡纳米粉体的溶液直接合成法.钛工业进展20 3.2003,20(3),25-27页. * |
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